Medical instrument with modified memory and flexibility properties and method

ABSTRACT

Medical instruments, particularly, endodontic instruments with unique limited memory characteristics, and methods for making such instruments. One embodiment includes heat treating a finished endodontic instrument. A related embodiment includes electropolishing a finished endodontic instrument and then heat treating the endodontic instrument.

CROSS-REFERENCE(S) TO RELATED APPLICATION(S)

This application claims priority to U.S. patent application Ser. No.12/950,536 entitled “Endodontic Instrument With Modified Memory andFlexibility Properties and Method” to Heath et al. filed on Nov. 19,2010, the content of which is incorporated herein by reference in itsentirety, and further claims priority to U.S. Provisional PatentApplication No. 61/263,192, entitled “Endodontic Instrument WithModified Memory and Flexibility Properties and Method” to Bennett et al.filed on Nov. 20, 2009, the content of which is incorporated herein byreference in its entirety.

FIELD

This disclosure relates to the field of medical instruments,manufacturing treatments, and methods of use therefor. Moreparticularly, this disclosure relates to medical instruments and methodsfor manufacturing and using such instruments to provide medicalinstruments and techniques with unique desired properties.

BACKGROUND

The present disclosure relates to endodontic instruments, orthodonticinstruments, other medical instruments, and to methods of making suchinstruments. Prior related medical instruments have been plagued withrecurrent problems including, but not limited to, undesired lateraltransportation in curved canals, difficulties with enlarging curvilinearcanals while substantially maintaining the original center axis of thecanals, and problems with binding and/or “screwing in” of prior NiTiinstruments in such canals during endodontic or orthodontic procedures.For these and other medical procedures, there is a need for handheldprobing, actuating, and/or surgical-type instruments with specificmetallurgical and behavioral properties.

SUMMARY

The above and other needs are met by a method for modifying a physicalcharacteristic of a medical instrument. The method comprises the stepsof placing a medical instrument (e.g., an endodontic instrument) in aheated environment having a temperature of from about 450° C. to about550° C. for from about 90 minutes to about 300 minutes, wherein themedical instrument is made from at least about 50% by mass of asuperelastic alloy. Preferably, the endodontic instrument comprises atapered endodontic instrument made of a nickel-titanium composition andconfigured as a file, rasp, broach, or other device for cleaning,scraping, extirpating, and/or debriding a root canal of a tooth. In oneembodiment, the instrument is placed in the heated environment for aperiod from about 120 minutes to about 150 minutes. In a relatedembodiment, the instrument is placed in the heated environment for aperiod from about 180 minutes to about 300 minutes. In one embodiment,the placing step further comprises placing the endodontic instrument ina heated gaseous environment having a gas temperature of from about 490°C. to about 510° C. wherein the gaseous environment preferably isambient air.

Preferably, the instrument undergoes a machining step to form a workingportion prior to placing the endodontic instrument in the heatedenvironment.

In one embodiment, the method for modifying a physical characteristic ofan endodontic instrument described above is made by further including astep of electropolishing the endodontic instrument prior to placing theendodontic instrument in the heated environment.

In one embodiment, the placing step further includes placing theendodontic instrument in a heated gaseous environment having a gastemperature of from about 490° C. to about 510° C. wherein the gaseousenvironment preferably is ambient air. The method further may include astep of electropolishing the endodontic instrument prior to placing theinstrument in the heated environment. In a preferred embodiment, theplacing step further includes a step selected from the group consistingof heat treating the endodontic instrument for at least 120 minutes ifthe endodontic instrument has a core diameter ranging from about1.9×10⁻² mm to about 3.1×10⁻² mm; heat treating the endodonticinstrument for from at least 120 minutes to about 240 minutes if theendodontic instrument has a core diameter ranging from about 3.1×10⁻² mmto about 4.8×10⁻² mm; or heat treating the endodontic instrument forfrom at least 240 minutes to about 300 minutes if the endodonticinstrument has a core diameter greater than about 4.8×10⁻² mm. In all ofthe embodiments, the instrument, after being exposed to the heatedenvironment, is preferably allowed to cool using natural heat transfermechanisms in ambient air.

In another aspect, embodiments of the disclosure provide an endodonticinstrument with modified memory characteristics, the endodonticinstrument made by the various method embodiments described above andincluding, for example, a method including the steps of placing anendodontic instrument in a heated environment having a temperature offrom about 450° C. to about 550° C. for from about 90 to about 300minutes, wherein the endodontic instrument is made from at least about50% by mass of a superelastic alloy. In one embodiment, the step ofplacing the endodontic instrument in a heated environment furthercomprises placing the endodontic instrument in the heated environmentfor from about 180 minutes to about 300 minutes.

BRIEF DESCRIPTION OF THE DRAWINGS

Further features, aspects, and advantages of the present disclosure willbecome better understood by reference to the following detaileddescription, appended claims, and accompanying figures, wherein elementsare not to scale so as to more clearly show the details, wherein likereference numbers indicate like elements throughout the several views,and wherein:

FIG. 1A shows a further somewhat schematic representation of a toothroot canal being operated on using a dental instrument;

FIG. 1B shows a somewhat schematic representation of a tooth beingoperated on using a dental instrument;

FIG. 2 shows a two-dimensional plot of torque data (vertical axis)versus angular deflection data (horizontal axis) for untreated(“control”) NiTi instruments;

FIG. 3 shows a two-dimensional plot of the data in FIG. 2 wherein thedata sets have been fitted to conform to third degree polynomialequation curves;

FIG. 4 shows a two-dimensional plot of torque data (vertical axis)versus angular deflection data (horizontal axis) for several NiTiinstruments treated according to one embodiment of the invention;

FIG. 5 shows a two-dimensional plot of torque data (vertical axis)versus angular deflection data (horizontal axis) for several NiTiinstruments treated according to another embodiment of the invention;

FIG. 6 shows a two-dimensional plot of torque data (vertical axis)versus angular deflection data (horizontal axis) for several NiTiinstruments treated according to a further embodiment of the invention;

FIG. 7 shows a two-dimensional plot of torque data (vertical axis)versus angular deflection data (horizontal axis) for several NiTiinstruments treated according to an additional embodiment of theinvention;

FIG. 8 shows a two-dimensional plot of the data in FIG. 7 wherein thedata sets have been fitted to conform to third degree polynomialequation curves;

FIG. 9 shows an apparatus used to test cyclical fatigue of a dentalinstrument;

FIG. 10 shows a two-dimensional plot of torque data (vertical axis)versus angular deflection data (horizontal axis) for twenty NiTiinstruments treated according to an embodiment of the invention;

FIG. 11 shows a two-dimensional plot of the data in FIG. 10 wherein thedata sets have been fitted to conform to third degree polynomialequation curves;

FIG. 12 shows the two-dimensional plot of torque data (vertical axis)versus angular deflection data (horizontal axis) shown in FIG. 11further including a superimposed curve generated from the average valuesof the coefficients for the third degree polynomial equations used tofit the data from FIG. 10 in the curves shown in FIG. 11;

FIG. 13 shows comparative cyclical fatigue measurements including thoseinvolving heat treated instruments with no prior electropolishing stepas compared to heat treated instruments that had undergone a priorelectropolishing step;

FIG. 14 shows comparative torque measurements including those involvingheat treated instruments with no prior electropolishing step as comparedto heat treated instruments that had undergone a prior electropolishingstep;

FIG. 15 shows comparative angular deflection measurements includingthose involving heat treated instruments with no prior electropolishingstep as compared to heat treated instruments that had undergone a priorelectropolishing step;

FIG. 16 shows comparative cyclical fatigue measurements including thoseinvolving nickel titanium instruments with no prior heat treatment orelectropolishing step (“NT”), heat treated instruments with no priorelectropolishing step (“NT+HT”), and heat treated instruments that hadundergone a prior electropolishing step (“NT+HT+EP”);

FIG. 17 shows comparative torque measurements including those involvingnickel titanium instruments with no prior heat treatment orelectropolishing step (“NT”), heat treated instruments with no priorelectropolishing step (“NT+HT”), and heat treated instruments that hadundergone a prior electropolishing step (“NT+HT+EP”);

FIG. 18 shows comparative angular deflection measurements includingthose involving nickel titanium instruments with no prior heat treatmentor electropolishing step (“NT”), heat treated instruments with no priorelectropolishing step (“NT+HT”), and heat treated instruments that hadundergone a prior electropolishing step (“NT+HT+EP”);

FIG. 19 shows the torn cross section of a heat treated endodonticinstrument after testing wherein the instrument had been heat treatedaccording to an embodiment of the invention prior to such testing;

FIG. 20 shows comparative cyclical fatigue measurements including thoseinvolving nickel titanium instruments with no prior heat treatment orelectropolishing step (“NT”), heat treated instruments with no priorelectropolishing step (“NT+HT”), heat treated instruments that hadundergone a prior electropolishing step (“NT+HT+EP”), andelectropolished instruments with no prior heat treatment step (NT+EP),and the respective average values of these categories shown by the largedashed rectangular bars around each respective group of smaller bars;

FIG. 21 shows comparative torque measurements including those involvingnickel titanium instruments with no prior heat treatment orelectropolishing step (“NT”), heat treated instruments with no priorelectropolishing step (“NT+HT”), heat treated instruments that hadundergone a prior electropolishing step (“NT+HT+EP”), andelectropolished instruments with no prior heat treatment step (NT+EP),and the respective average values of these categories shown by the largedashed rectangular bars around each respective group of smaller bars;

FIG. 22 shows comparative angular deflection measurements includingthose involving nickel titanium instruments with no prior heat treatmentor electropolishing step (“NT”), heat treated instruments with no priorelectropolishing step (“NT+HT”), heat treated instruments that hadundergone a prior electropolishing step (“NT+HT+EP”), andelectropolished instruments with no prior heat treatment step (NT+EP),and the respective average values of these categories shown by the largedashed rectangular bars around each respective group of smaller bars;

FIG. 23A shows comparative cyclical fatigue measurements including thecombined measurements of heat treated NiTi instruments with no priorelectropolishing step (“HT”) and electropolished instruments with noprior heat treatment step (“EP”), the sum of which are designated as “HT& EP (separate instruments; combined data)”; versus heat treatedinstruments that also underwent a prior electropolishing step, suchinstruments designated as “EP+HT (same instrument)”; the respectiveaverage values of these categories shown by the large dashed rectangularbars around each respective group of smaller bars;

FIG. 23B shows comparative torque measurements including the combinedmeasurements of heat treated NiTi instruments with no priorelectropolishing step (“HT”) and electropolished instruments with noprior heat treatment step (“EP”), the sum of which are designated as “HT& EP (separate instruments; combined data)”; versus heat treatedinstruments that also underwent a prior electropolishing step, suchinstruments designated as “EP+HT (same instrument)”; the respectiveaverage values of these categories shown by the large dashed rectangularbars around each respective group of smaller bars

FIG. 23C shows comparative angular deflection measurements including thecombined measurements of heat treated NiTi instruments with no priorelectropolishing step (“HT”) and electropolished instruments with noprior heat treatment step (“EP”), the sum of which are designated as “HT& EP (separate instruments; combined data)”; versus heat treatedinstruments that also underwent a prior electropolishing step, suchinstruments designated as “EP+HT (same instrument)”; the respectiveaverage values of these categories shown by the large dashed rectangularbars around each respective group of smaller bars; and

FIG. 24 shows a side view of a kit including a plurality of apexlocating dental tools according to one embodiment of the presentinvention.

DETAILED DESCRIPTION

Various terms used herein are intended to have particular meanings. Someof these terms are defined below for the purpose of clarity. Thedefinitions given below are meant to cover all forms of the words beingdefined (e.g., singular, plural, present tense, past tense). If thedefinition of any term below diverges from the commonly understoodand/or dictionary definition of such term, the definitions belowcontrol.

mN·m: the unit symbol for milli-Newton·meter.

m: the length unit symbol for meter.

mm: the length unit symbol for millimeter.

Working portion: That part of an endodontic instrument which includessurface features for removing material from a root canal including, butnot limited to, surface features for scraping, shaving, cutting,penetrating, excavating, and/or removing material from canal wallsurfaces in an effort to shape and/or enlarge a root canal.

FIGS. 1A and 1B show somewhat schematic representations of a tooth 10including a natural root canal 12 in which an endodontic instrument 14is being used to extirpate the natural root canal 12. When devices suchas the endodontic instrument 14 shown in FIG. 1A are made fromnickel-titanium (or “NiTi” or “Nitinol”), such devices tend to haveimproved flexibility properties relative to similar devices made ofstainless steel. This property of NiTi and other similar alloys issometimes referred to in part as superelasticity or psuedoelasticity andis often lauded as a unique and beneficial characteristic of endodonticfiles made from NiTi.

As FIG. 1A shows, however, when NiTi endodontic devices such as taperedfiles are used to navigate, for example, the natural root canal 12 ofthe tooth 10, the tendency of the device 14 to veer to a path contraryto the natural root canal 12 shape is a continuous concern for a dentalpractitioner—particularly when the instrument is used along a naturalroot canal with excessive curvature. A first deviation path 16 and asecond deviation path 18 are shown in FIG. 1A to illustrate the mannerin which an instrument made of NiTi tends to create disproportionatelateral forces along an inner surface 20 of the natural root canal 12 atcertain locations. If this tendency is not carefully monitored by adental practitioner, such instrument could easily (and often does)deviate from the natural root canal 12, boring an artificial structurewhich has the potential to compromise an entire tooth structure.

In an attempt to address the drawbacks associated with NiTi dentalinstruments as used in endodontic procedures discussed above, theinventor has performed a number of experiments in an effort to increasethe beneficial flexibility properties of NiTi which, in turn, decreasesthe lateral forces exerted by a NiTi dental instrument on the innersurface of a tooth root canal. The inventor has surprisingly found amethod for treating machined NiTi instruments that increases theflexibility of such instruments.

In a first study, the Applicant performed twenty five tests using ADAguidelines (discussed infra) on five groups of endodontic files forproperties including torque and angular deflection to see if variousheat treatment methods had any effect on the relative performance of thefiles. Trends of interest became apparent based on the visual“signature” of each set of data sets. Table 1 below indicatesrelationships between each group of tests with various parameters.

TABLE 1 Ave. Torque Ave. Angular Deflection (mN · m) (Revolutions)Control Group about 2 1.61 Experimental Group 1 less than 2 2.89Experimental Group 2 unstable data 3.32 Experimental Group 3 unstabledata 3.69 Experimental Group 4 about 2 4.05

Graphs shown in FIGS. 2-8 plot torque (vertical axis) versus angulardeflection (horizontal axis). In each of the graphs shown in FIGS. 2-8,240 measurement samples for torque versus angular deflection were takenper one full axial (twisting) revolution of the instrument. FIG. 2 showsa graph of four data sets representing four separate test samplesincluded in the control group which included only NiTi instruments thathad not been heat treated according to Applicant's treatment method. Afifth data set in the control group was discarded because of a testingfault with the sample. As can be seen in FIG. 2, all of the test runs ofthe control group displayed a similar graphical signature which is moreeasily seen in FIG. 3 wherein the data associated with each test samplewas used to generate a second order polynomial trend line.

Each of FIGS. 4-8 show data sets of wire samples that have been heattreated by being placed in a stainless steel pan and inserted into anoven which was pre-heated to about 500° C. The difference between theexperimental groups was the amount of time the test samples of aparticular group were kept in the oven. FIG. 4, for example, shows agraph of five data sets representing five separate test samples includedin the first experimental group which remained in the oven for 15minutes. FIG. 5 shows a graph of five data sets representing fiveseparate test samples included in the second experimental group whichremained in the oven for 45 minutes. FIG. 6 shows a graph of five datasets representing five separate test samples included in the thirdexperimental group which remained in the oven for 90 minutes. FIG. 7shows a graph of five data sets representing five separate test samplesincluded in the fourth experimental group which remained in the oven for120 minutes. FIG. 8 shows second order polynomial trend lines based onthe data sets of the fourth experimental group so that the respective“signatures” of these data sets can be more clearly seen relative to oneanother.

Although the average torque value of the fourth experimental group wasvery similar to the average torque value of the control group, it wassurprisingly discovered that the average angular deflection of thefourth experimental group demonstrated an increase of almost 250%relative to the average angular deflection of the control group.Additionally, the samples tested in the fourth experimental groupdemonstrated a cyclical fatigue of about 120 seconds as compared toabout 30 seconds as demonstrated with respect to the samples tested inthe control group. Also, the visual signatures of the individual datasets in FIG. 7 and FIG. 8 were more precisely aligned as best shown inFIG. 8. As a follow-up to the test results given above, more testing wasperformed with a focus on heating machined endodontic NiTi instrumentsas described above for about 120 minutes and gathering additional data.

The purpose of the additional analysis was to build upon theexperimentation discussed above in which the inventor was able to modifycertain physical properties of Nickel-Titanium through a specificheating process. Some goals for the additional tests are shown below inTable 2.

TABLE 2 TEST ITEM NAME CRITERIA ACCEPTANCE 1 Torque 1.77 Minimum Mustpass Minimum Criteria per ADA 101 2 Angular Deflection 360° Minimum Mustpass Minimum Criteria per ADA 101 3 Cyclical Fatigue 10-Series Must begreater than Equivalent Industry equivalence 4 Flexibility 10-SeriesMust be less than Equivalent Industry equivalence 5 Clinician FeedbackInquiry Positive Feedback

The additional testing followed the guidelines found in ADA no. 28(sections 6.4 and 6.5), ADA no. 101, and ISO 3630-1 (sections 7.4 and7.5), the contents of which are incorporated herein by reference intheir entireties. Cyclical fatigue testing is not an ISO standard test,but it has been utilized in the testing of rotary Nickel-Titaniuminstruments over the past few years. Such cyclical fatigue testingincludes a motor unit 22 as shown in FIG. 9 set at, for example, about300 rpm to simulate the speed of an instrument as used during, forexample, a root canal procedure. A Ni—Ti test instrument is lowered intoa simulated canal structure 24 which may be set at about 90° relative tothe plane of rotation of the test instrument, until the depth of acalibration line along the test instrument is reached at, for example,about 19 millimeters in reference to a first end 26 of the simulatedcanal structure 24. The amount of time the test instrument is rotatedprior to breaking or otherwise failing is recorded so as to determinehow long it took, under controlled conditions, for the test instrumentto break.

No less than twenty machined endodontic NiTi instruments which had beenheat treated in a 500° C. oven for about 120 minutes were testedaccording to the criteria set forth above in Table 2. More specifically,the tested instruments were 10 Series™ endodontic files offered by D&SDental, LLC of Johnson City, Tenn., the files having a total length ofabout 25 mm, a working length of about 10 mm, and a taper rate of 0.04mm/mm. An important aspect of the method described herein is heattreating after machining of a NiTi dental instrument has a profoundeffect on the physical properties of the machined instrument. Table 3Abelow summarizes the test results.

TABLE 3A ITEM NAME CRITERIA RESULTS COMMENTS 1 Torque 1.77 mN · m WorstCase Passed Minimum 4 mN · m. 2 Angular 360° Worst Case PassedDeflection Minimum 510° 3 Cyclical 10-Series Mean of 160.79 PassedFatigue 25 seconds seconds with a @ 90° Standard Deviation of 38 seconds4 Flexibility 10-Series Mean of 18 5 pieces were 50 mN · m mN · m @ 45°tested for amount @ 45° of torque needed to reach 45°. Passed 5Clinician Inquiry Pros: Good Cutting Marginal Feedback ability, Nobreakage Cons: Too flexible, loss of tactile feel

The test results overall showed notable improvement in all categorieslisted in Table 3A. Table 3B shows specific product comparisons betweendifferent brands of endodontic instruments. The torque measurements forinstruments treated using the method described above were all still wellabove the minimum standards set forth in ADA no. 28 (sections 6.4 and6.5), ADA no. 101, and ISO 3630-1 (sections 7.4 and 7.5).

TABLE 3B With CM ™ Without CM ™ Process Torque (mN · m) Process Torque(mN · m) 10-Series 25_04 4.4995 10-Series 25_04 7.0307 10-Series 40_0413.3086  10-Series 40_04 21.9641  Typhoon 25_04 1.6006 Typhoon 25_043.1405 Typhoon 40_04 5.2195 Typhoon 40_04 9.4911 (no data) (no data)Twisted 25_04 1.4918 (no data) (no data) Twisted 40_04 3.4895 (no data)(no data) Vortex 25_04 3.3289 (no data) (no data) Vortex 40_04 9.7674

The graph shown in FIG. 10 shows the twenty samples as plotted withrespect to torque (vertical axis) versus angular deflection wherein 240data measurements were taken per one 360° (axial) revolution of a testedsample. FIG. 11 shows trendlines plotted based on third order polynomialequations to best model the data results for each test sample. FIG. 12shows the trendlines from FIG. 11 along with a bold trendline generatedand plotted based on the average values of the twenty trend linesrepresenting each test sample. Table 4 shows the model equations used togenerate each trendline in FIG. 11 as well as the equation used togenerate and plot the bold trendline in FIG. 12.

TABLE 4 Coefficients as used in a third order polynomial equation f(x) =Ax³ + Bx² + Cx + D. Test Coefficients Sample A B C D 1 −0.00000008−0.000004 0.0271 4.4365 2 −0.00000008 −0.000005 0.0291 4.4036 3−0.0000001 0.00002 0.0152 4.4996 4 −0.0000001 −0.000004 0.0346 4.7673 5−0.00000002 −0.00004 0.0321 4.8333 6 −0.00000005 −0.000007 0.0195 4.71317 −0.00000008 −0.0000006 0.0253 4.3494 8 0.00000007 −0.0001 0.04914.2493 9 −0.00000008 −0.000005 0.0314 4.2093 10 −0.0000001 0.000040.0182 4.3039 11 −0.0000001 −0.000007 0.0305 4.6517 12 −0.00000008−0.000002 0.0252 4.6123 13 −0.0000002 0.00003 0.03 4.6047 14 −0.00000002−0.00002 0.0224 4.7004 15 0.00000003 −0.00006 0.0287 4.5002 16−0.00000007 −0.000003 0.0243 4.5967 17 −0.0000003 0.00008 0.0209 5.06318 0.00000002 −0.00006 0.038 4.2322 19 −0.0000002 0.00006 0.0285 4.787320 −0.00000006 −0.00003 0.033 4.9694

Based on the results of the follow-up tests, the average torque valuefor the samples tested was about 4.57 mN·m. The average number ofmeasurements taken prior to instrument failure was 372.5 whichcorresponds to about 1.5 full axial revolutions (i.e., 372.5measurements÷240 measurements per axial revolutions). The values areshown in FIG. 12.

The results of the tests carried out above are promising because theydemonstrate that heat treating an endodontic instrument to about 500° C.for about two hours or more after machining has taken place results inimproved instrument flexibility. Such increased flexibility leads to aninstrument such as the treated instrument 14′ shown in FIG. 1B to moreclosely follow the natural root canal 12 of the tooth 10 and exhibitless lateral forces along the inner surface of such root canal 12.

One specific example of improved cyclical fatigue is shown in FIG. 19showing the torn cross section of a heat treated endodontic instrumenttested at a speed 300 rpm, and dry (i.e., no irrigation solution). Thistesting was conducted for Applicants by the Department of OralBiological & Medical Sciences at the University of British Colombia inVancouver, British Colombia. The micrographs show that the instrumentfractured, but a small portion 28 of the instrument held together andmaintained the integrity of the instrument for an extended period oftime such that the test lasted for over 3000 cycles. Typical NiTiinstruments usually completely separate upon a relatively small fractureoccurs, but the heat treated instrument shown in FIG. 19 behaveddifferently and maintained its integrity with a large and deep fracturefor more than enough time for a user to have realized that theinstrument was mechanically failing.

The improved cyclical fatigue measurements (as compared to untreatedNiTi instruments) strongly suggests that endodontic instruments treatedaccording to embodiments described herein will last longer and enduremore stress prior to failing. This enhancement translates into less timespent extracting broken bits of instruments and more time accomplishingthe goal of a particular endodontic procedure.

In one embodiment, a method is disclosed for treating medicalinstruments including placing a medical instrument into an environmentheld at least at about 450° C. to about 550° C., more preferably fromabout 475° C. to about 525° C., and most preferably from about 490° C.to about 510° C. for a period of from about 90 minutes to about 180minutes and more preferably from about 120 minutes to about 150 minutes.The dental instrument is preferably an endodontic instrument made fromat least about 50% of a superelastic alloy, and the instrument ispreferably a file, reamer, or a broach. Alternatively, the dentalinstrument can also include a plugger or a spreader. As anotheralternative, the dental instrument can include an orthodontic tool,wire, and/or appliance. The superelastic alloy is preferablyNickel-Titanium. The heat treated medical instrument preferably isplaced in a metal pan with freedom of movement during the heating step.In this and other related embodiments, no special treatment atmosphereis required and, in a preferred embodiment, simple air is used.Similarly, unlike other processes that require special quenching stepsto obtain desired properties, Applicants' embodiments require noquenching steps. Heated instruments are preferably brought to ambientair temperature by natural conduction, convection, and radiation heattransfer.

Applicants have determined that the duration of heat treatment describedherein is preferably a function of the core diameter of the instrumentbeing treated. For example, instruments with core diameters ranging fromabout 1.9×10⁻² mm to about 3.1×10⁻² mm are preferably heat treated forat least 120 minutes; instruments with core diameters ranging from about3.1×10⁻² mm to about 4.8×10⁻² mm are preferably heat treated for from atleast 120 minutes to about 240 minutes; and instruments with corediameters greater than about 4.8×10⁻² mm are preferably heat treated forfrom at least 240 minutes to about 300 minutes. These ranges overlapsomewhat because other factors also determine the effectiveness the heattreatment process including, for example, the particular helix angle(s)of an endodontic instrument.

In a related embodiment, flexibility of an elongate machined medicalinstrument is varied along its length axis by heat treating only one ormore discrete portions of the medical instrument. In the followingexamples, it is to be assumed that the medical instrument is anendodontic instrument including a working portion approximately 10 mm inlength, such 10 mm length including a distal end (tip) and a flutelength end (rear), wherein the second end is adjacent a non-workingportion of the endodontic instrument. The assumptions given herein arefor illustrative purposes only and are not intended as a limitation onthe technology as described herein.

In a first example, an endodontic instrument made from primarily asuperelastic alloy such as NiTi may be selectively heat treated alongabout 2 mm adjacent the distal end (tip) of the instrument, resulting inan instrument with a tip having enhanced flexibility with the remainderof the instrument remaining relatively rigid.

In another example, an endodontic instrument made from primarily asuperelastic alloy such as NiTi may be selectively heat treating adiscrete cross section of an instrument having a length of about 1 mm toabout 2 mm located about 5 mm from the tip of the instrument. This willresult in a relatively rigid tip, flexible middle portion, andrelatively rigid end portion of the working portion of the instrument.

In yet another example, an instrument is heat treated from the tip ofthe instrument to about 2 mm from the tip as well as heat treated fromabout 9 mm to about 10 mm from the tip of the instrument. This examplewould result in an instrument with relative flexibility near the tip,relative rigidity along a midsection of the working portion of theinstrument (i.e., from about 3 mm from the tip to about 8 mm from thetip), and relative flexibility from about 9 mm to about 10 mm from thetip of the instrument.

In another example illustrated in FIG. 20, an instrument such as an apexlocating apparatus is heat treated from the tip of the instrument toabout 4 mm to about 5 mm from the tip. This example would result in aninstrument with relative flexibility near the tip. In an apex locatingapparatus, the relative flexibility of the tip allows the tip of theapparatus to more gingerly navigate the root canal of a tooth to locatethe apical foramen of such tooth without puncturing through or beyondthe canal itself.

FIG. 20 shows an example of a kit 40 of endodontic tools, the kit 40 inFIG. 20 including a plurality of endodontic tools 42 (42A-42D) havingvarying sizes and shapes for conforming to various root canal profiles.The plurality of endodontic tools 42 have controlled memory propertiesas a result of their NiTi composition and the manner in which theendodontic tools have been treated according to the treatment methodsdiscussed above, along a memory section 44 of each endodontic tool. Thememory section 44 preferably ranges from the tip of each tool to about 4mm to about 10 mm from the tip of each tool. As illustrated in FIG. 20,a first endodontic tool 42A and a second endodontic tool 42B in the kit40 have substantially constant diameters (shown as 46A and 46B). A thirdendodontic tool 42C and a fourth endodontic tool 42D have tapereddiameters (shown as 46C and 46D). The tapered diameter 46C of the thirdendodontic tool 42C preferably ranges from about 0.005 mm/mm to about0.015 mm/mm, and most preferably is about 0.01 mm/mm. The tapereddiameter 46D of the fourth endodontic tool 42D preferably ranges fromabout 0.01 mm/mm to about 0.03 mm/mm, and most preferably is about 0.02mm/mm. The endodontic tools 42 each preferably have a memory section 50(50A-50D), the memory section preferably ranging in length from at leastabout 4 mm to about 12 mm from the tip of the endodontic tool. Theendodontic tools 42 also preferably have a pointed tip section 52(52A-52D) to enable each tool to reach the apical foramen of a tooth.The pointed tip section 52 preferably has an angle λ ranging from about20° to about 40° and most preferably an angle of about 30°.

Other discrete treatment options are contemplated herein for treatmentof specific axial cross-sections of an endodontic instrument to effectspecific physical property alterations along the instrument's length asdesired. The specific treatment may be accomplished using focused energyat certain points along an endodontic instrument and/or placing aresistance forming layer or layers on sections of an instrument that arenot to be heat treated.

In addition to the treated endodontic instruments and related methodsdescribed above, a related embodiment includes a step ofelectropolishing an endodontic instrument prior to the various heattreatments described above. Electropolishing is a technique that hasbeen used in the art for the purpose of removing surface flaws inendodontic instruments. However, Applicants have surprisingly found thatelectropolishing an endodontic instrument prior to heat treating theendodontic instrument as described above results in improved instrumentcharacteristics.

Applicants tested ten pieces of 0.25/0.04 (size/taper rate) Typhoonbrand endodontic instruments in May 2010. The test results indicatedsubstantially improved cyclical fatigue at 60° (angular), improvedtorque, and improved angular deflection when compared to similarly heattreated endodontic instruments that were not electropolished prior toheat treatment. The results are summarized below in Table 5, andgraphically shown in FIGS. 13-15 wherein FIG. 13 shows the comparativecyclical fatigue measurements, FIG. 14 shows the comparative torquemeasurements, and FIG. 15 shows the comparative angular deflectionmeasurements. The parameters used for the testing included use of a EsmaElectro-polishing machine with E272 Acid wherein the temperature of theacid was kept at about 80° C. Each run lasted approximately 240 secondsand approximately 25 volts of DC power was applied through the positiveand negative circuits of the electro-polishing machine.

TABLE 5 COMMENTS ITEM NAME CRITERIA RESULTS N Mean StDev SE Mean 1Cyclical Past product Must be greater Cyclical CM 7 76.0 16.8 6.4Fatigue @ 60° group comparison than control group Cyclical EP 5 370.061.6 28 2 Torque Past product Must be greater Torque CM 9 1.613 0.2880.096 group comparison than control group Torque EP 5 4.261 0.946 0.42 3Angular Past product Must be greater AD CM 10 549.8 58.3 18 Deflectiongroup comparison than control group AD EP 5 1370 146 65

Applicants further tested at least five different groups ofnickel-titanium endodontic instruments wherein some had not been heattreated, some had been treated without a prior electropolishing step,some had been electropolished without a prior heat treating step, andthe remainder were heat treated with a prior electropolishing step. Thecomparative data is shown in Table 6 below as well FIGS. 16-18 whereinFIG. 16 shows comparative cyclical fatigue, FIG. 17 shows comparativetorque measurements, and FIG. 18 shows comparative angular deflectionmeasurements.

TABLE 6 Cyclical Fatigue Torque Angular Deflection NT + HT NT + EP + HTNT NT + HT NT + EP + HT NT NT + HT NT + EP + HT NT 72 298 37 2.1582519755.09347466 1.329483217 975 1428 569 63 462 46 1.346749233 2.831626591.519409391 1012 1241 498 108 333 34 1.674803533 3.78125746 2.244582054969 1205 647 76 377 24 1.571207438 4.67909028 3.263276987 1283 1413 61759 380 43 1.761133612 4.9208145 4.40283403 1146 1561 506 NT =Nickel-Titanium instrument HT = Heat treatment step EP =Electropolishing step

Based on the results shown in FIGS. 13-18, Table 5, and Table 6, thisdisclosure further includes a method for treating medical instrumentsincluding electropolishing a medical instrument; and placing a medicalinstrument into an environment held at least at about 450° C. to about550° C., more preferably from about 475° C. to about 525° C., and mostpreferably from about 490° C. to about 510° C. for a period of fromabout 90 minutes to about 180 minutes and more preferably from about 120minutes to about 150 minutes. The dental instrument is preferably anendodontic instrument made from at least about 50% of a superelasticalloy, and the instrument is preferably a file, reamer, or a broach.Alternatively, the medical instrument can include an orthodontic tool,wire, and/or appliance. The superelastic alloy is preferablyNickel-Titanium. The heat treated medical instrument preferably isplaced in a metal pan with freedom of movement during the heating step.

FIG. 20 shows the average relative improvements in cyclical fatigue,torque, and angular deflection provided by the electropolishing stepalone; FIG. 21 shows the average relative improvements in cyclicalfatigue, torque, and angular deflection provided by the heating stepalone; and FIG. 22 shows the average relative improvements in cyclicalfatigue, torque, and angular deflection wherein both a heating step andelectropolishing step were performed on the same instruments.

TABLE 7 Cyclical Fatigue Torque Angular Deflection NT + HT NT + EP + HTNT NT + EP NT + HT NT + EP + HT NT NT + EP NT + HT NT + EP + HT NT NT +EP 72 298 37 44 2.158252 5.09347466 1.33 3.107883 975 1428 569 803.87 63462 46 32 1.346749 2.83162659 1.52 3.246011 1012 1241 498 724.25 108 33334 37 1.674804 3.78125746 2.24 2.330912 969 1205 647 601.05 76 377 24 371.571207 4.67909028 3.26 4.005716 1283 1413 617 785.24 59 380 43 371.761134 4.9208145 4.4 2.607168 1146 1561 506 609.84 NT =Nickel-Titanium instrument HT = Heat treatment step EP =Electropolishing step

FIGS. 23A-23C show the results of the cumulative HT and EP data fromFIGS. 20-22 and the net effect of separately combined HT and EP dataversus the synergistic effect of treating the same instrument with bothan electropolishing step and a heating step. In FIGS. 23A-23C, thebaseline data for NiTi is subtracted out in each instance to moreclearly show that when both heating and electropolishing steps areperformed on the same instruments versus the combined data of separatelytreated batches of instruments wherein one batch were heat treated andthe other were treated by electropolishing techniques, the instrumentsthat underwent both electropolishing and heat treatment demonstratednotably superior results. This deviation demonstrates a synergisticeffect when instruments as described herein are both heat treated andelectropolished versus being heat treated without an electropolishingstep. The dashed rectangular boxes in FIGS. 20-22 and 23A-23C representaverage values and provide a clearer picture of how the electropolishingstep and the heating step together provide a synergistic improvingeffect on all of the tested categories including cyclical fatigue,torque, and angular deflection when compared to merely heating alone orelectropolishing alone.

In addition to the treated medical instruments and related methodsdescribed above, another embodiment involves forming a heat treated NiTiinstrument to a particular shape and returning the instruments to itsoriginal shape after the application of sufficient heat. In one example,an endodontic instrument made from a primarily superelastic alloy suchas NiTi may be deformed by, for example, an endodontic surgeon to fit aparticular use. One specific example includes forming a dental obturatorto a particular shape for filling a root canal with sealing materials.After the endodontic instrument is used for the particular purpose, itmay be heated to at least its transformation temperature at which pointthe instrument returns to its initial, undeformed shape. Additionally,this process of deforming and returning the instrument to its originalundeformed shape may be used for other endodontic and orthodonticinstruments. These steps can also be used, for example, with respect tothe kit 40 including a plurality of endodontic tools 42 shown in FIG.24.

The foregoing description of preferred embodiments of the presentdisclosure has been presented for purposes of illustration anddescription. The described preferred embodiments are not intended to beexhaustive or to limit the scope of the disclosure to the preciseform(s) disclosed. Obvious modifications or variations are possible inlight of the above teachings. The embodiments are chosen and describedin an effort to provide the best illustrations of the principles of thedisclosure and its practical application, and to thereby enable one ofordinary skill in the art to utilize the concepts revealed in thedisclosure in various embodiments and with various modifications as aresuited to the particular use contemplated. All such modifications andvariations are within the scope of the disclosure as determined by theappended claims when interpreted in accordance with the breadth to whichthey are fairly, legally, and equitably entitled.

What is claimed is:
 1. A method for modifying a physical characteristicof a medical instrument, the method comprising the steps of placing amedical instrument in a heated environment having a temperature of fromabout 450° C. to about 550° C. for from about 180 minutes to about 300minutes, wherein the medical instrument is made from at least about 50%by mass of a superelastic alloy, and wherein the medical instrumentcomprises an endodontic instrument.
 2. The method of claim 1 wherein theplacing step further includes placing the medical instrument in a heatedgaseous environment having a gas temperature of from about 490° C. toabout 510° C.
 3. The method of claim 1 wherein the heated environmentcomprises air.
 4. The method of claim 1 further comprising the step ofmachining the medical instrument to form a working portion prior toplacing the medical instrument in the heated environment.
 5. The methodof claim 1 further comprising the step of placing a resistance layeralong a first section of the medical instrument prior to placing themedical instrument in the heated environment, wherein the resistancelayer prevents the first section from undergoing the same degree of heattreatment in the heated environment as the remaining portions of themedical instrument that were not covered by the resistance layer.
 6. Themethod of claim 5 wherein the first section comprises all of the medicalinstrument except for from about 6 mm to no less than 4 mm from aterminus of a tapered end of the medical instrument.
 7. The method ofclaim 5 further comprising a step of electropolishing the medicalinstrument prior to placing the medical instrument in the heatedenvironment.
 8. The method of claim 1 further comprising a step ofelectropolishing the instrument prior to placing the instrument in theheated environment.
 9. The method of claim 1 wherein the placing stepfurther comprises heat treating the medical instrument for from at least240 minutes to about 300 minutes if the medical instrument has anaverage core diameter greater than about 4.8×10⁻² mm.
 10. The method ofclaim 1 further comprising the step of cooling the heated instrumentusing natural heat transfer mechanisms in ambient air.